Method of producing high bulk density molybdenum oxychloride

a molybdenum oxychloride and high bulk density technology, applied in the direction of chemically reactive gases, coatings, crystal growth processes, etc., can solve the problems of difficult handling, low vapor pressure, and low molybdenum pentachloride (moclsub>5/sub>), and achieve low bulk density, easy handling, and high bulk density

Pending Publication Date: 2021-01-14
JX NIPPON MINING& METALS CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

[0030]According to the method of the present invention, it is possible to achieve a higher bulk density of the crystals of molybdenum oxychloride having a low bulk density which was synthesized according to a general synthesizing method, and it becomes easier to handle such as the storage and transport. Moreover, the surface area of the crystals can be reduced based on such higher bulk density, and the hygroscopicity resistance and chemical stability can also be improved. Furthermore, it is also possible to simultaneously reduce impurities and improve the purity level based on the refining effect of sublimation. Based on these effects, it is possible to improve the operability of deposition and chemical reaction, as well as improve the performance and characteristics of the produced thin film and compound.

Problems solved by technology

Nevertheless, molybdenum pentachloride (MoCl5), which is a general molybdenum chloride, is difficult to handle as it is unstable and spontaneously generates toxic hydrogen chloride when decomposed, and there are problems related to the preservation and storage thereof for use in industrial processes.
While this kind of problem will not arise with CVD or ALD which uses metallic carbonyl as the raw material, carbonyl of metal including molybdenum has a low vapor pressure, and there is a problem in that the control of the raw material gas flow rate and pressure during CVD or ALD deposition is difficult.
If an organic metal compound of a specific structure is used, it is possible to exhibit a moderate vapor pressure as the raw material for use in CVD or ALD deposition, but because time and cost are required for synthesizing an organic metal compound of such a specific structure, there is a problem in that the cost will increase as the raw material of CVD or ALD deposition for use in industrial processes.
Nevertheless, the synthesized molybdenum oxychloride is a fluffy, extremely light floccose powder crystal, has a low bulk density, and there is a problem in that the handling thereof in its original form is difficult and inconvenient.

Method used

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  • Method of producing high bulk density molybdenum oxychloride

Examples

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example 1

[0064]By using the MoO2Cl2 obtained in Comparative Example 1 as the raw material, the method of the present invention, including sublimation / reaggregation, was applied in a reduced-pressure atmosphere. Here, the device having the configuration of FIG. 2(b) was used to perform the sublimation / reaggregation of the MoO2Cl2. The MoO2Cl2 as the raw material was held in a raw material holding container of a sublimation device, and this was connected to one end of a reaction tube made of glass. The inside of the sublimation device was depressurized by being exhausted from the side while maintaining the other end of the reaction tube in a state where the inside of the tube can be observed from the upper part. In Example 1, the pressure inside the device was set to 1 kPa. In this state, the MoO2Cl2 in the raw material holding container was gradually heated, and held at a heating temperature of 95° C. in which the raw material can be stably sublimated. When this state is maintained, the MoO2C...

example 2

[0065]The pressure inside the device was set to 5 kPa, and the raw material MoO2Cl2 was subject to sublimation / reaggregation in the same manner as Example 1. In Example 2, the temperature that the raw material MoO2Cl2 can be stably sublimated was 117° C., and the heating temperature of the raw material MoO2Cl2 was held at this temperature. Here, the temperature of the reaggregated part was 97° C. In this state, the sublimation / reaggregation of the MoO2Cl2 was performed until the sublimated sediment no longer increased based on visual observation while adjusting the position in the reaction tube where the reaggregated MoO2Cl2 is accumulated. Finally, when the MoO2Cl2 accumulated in the reaction tube was cooled and thereafter collected, it became separated from the inner wall of the reaction tube with relatively weak force, and could be easily recovered. FIG. 5 shows the appearance of the MoO2Cl2 obtained in Example 2. The MoO2Cl2 obtained in Example 2 had a bulk density of 1.1 g / cm3,...

example 3

[0066]The pressure inside the device was set to 20 kPa, and the raw material MoO2Cl2 was subject to sublimation / reaggregation in the same manner as Example 1. In Example 3, the temperature that the raw material MoO2Cl2 can be stably sublimated was 135° C., and the heating temperature of the raw material MoO2Cl2 was held at this temperature. Here, the temperature of the reaggregated part was 115° C. In this state, the sublimation / reaggregation of the MoO2Cl2 was performed until the sublimated sediment no longer increased based on visual observation while adjusting the position in the reaction tube where the reaggregated MoO2Cl2 is accumulated. Finally, when the MoO2Cl2 accumulated in the reaction tube was cooled and thereafter collected, the sediment tended to become hard and affixed to the inner wall of the reaction tube, and much effort was required for collecting the MoO2Cl2 in comparison to Examples 1 and 2. FIG. 6 shows the appearance of the MoO2Cl2 obtained in Example 3. The Mo...

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Abstract

Provided is a method of producing a high purity molybdenum oxychloride by including means of sublimating and reaggregating a raw material molybdenum oxychloride in a reduced-pressure atmosphere, or means of retaining a gaseous raw material molybdenum oxychloride, which was synthesized in a vapor phase, in a certain temperature range, and thereby growing crystals to obtain a higher purity molybdenum oxychloride having a high bulk density and high hygroscopicity resistance.

Description

TECHNICAL FIELD[0001]The present invention relates to a method of producing a high bulk density molybdenum oxychloride that can be suitably applied to a material for vapor phase growth of thin films or a catalyst for chemical reactions.BACKGROUND ART[0002]As thin films for use as contact plugs, wires and diffusion barrier layers under such wires in functional electronic devices such as semiconductor devices, low-resistance metal materials that are physically and chemically stable, such as molybdenum (Mo) and tungsten (W), have been often used from the past. As the diffusion barrier layer, thin films of compounds such as nitrides and carbides of these metals, are also often used.[0003]Other than for use as a diffusion barrier layer of electronic devices, for instance, a molybdenum disulfide (MoS2) thin film, which is a sulfide of molybdenum, has also been conventionally used as a lubricant layer at the sliding part of mechanical components. In recent years, an ultrathin two-dimension...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C01G39/00
CPCC01G39/00C23C16/45553C01P2004/45C01P2006/80C01P2006/10C30B23/066C30B23/002C30B25/16
Inventor TAKAHASHI, HIDEYUKI
Owner JX NIPPON MINING& METALS CORP
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